反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-Chlorobenzenesulphonyl chloride (1.17 g) was added portionwise to a solution of 4-(5-aminopyrid-2-yl)butanoic acid (1 g) in pyridine (15 ml). The resulting solution was allowed to stand at room temperature overnight when the solvent was removed under reduced pressure. The residue was dissolved in dilute sodium hydroxide solution (50 ml) and extracted with chloroform (4×50 ml) and the chloroform extracts were discarded. The aqueous layer was adjusted to pH=4 and was extracted with chloroform (3×100 ml). The chloroform extracts were dried over magnesium sulphate, the solvent was removed and residue was recrystallised from acetonitrile/water 1:1 to give the title compound (0.7 g) as white plates. m.p. 178°-180° C.
WORKUP
后处理
- customwhen the solvent was removed under reduced pressure
- dissolutionThe residue was dissolved in dilute sodium hydroxide solution (50 ml)
- extractionextracted with chloroform (4×50 ml)
- extractionwas extracted with chloroform (3×100 ml)
- dry with materialThe chloroform extracts were dried over magnesium sulphate
- customthe solvent was removed
- customresidue was recrystallised from acetonitrile/water 1:1